Contribution of EBSD for the Microstructural Study of Archaeological Iron Alloy Artefacts from the Archaeological Site of Loiola (Biscay, Northern Spain)

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

Dear authors,

The manuscript you presented deals with an interesting and important subject. It provides a simple but effective study on the microstructure of Roman-period iron artefacts using metallographic observation methods (etching, OM, and SEM), Electron Backscatter Diffraction (EBSD), microhardness measurements, and Raman microspectroscopy for phase identification, especially within inclusions.

Considering the potential impact on the field of studies, I believe this paper deserves publication. However, there are issues that the authors may wish to evaluate before being accepted for publication.

 

ABSTRACT: in my opinion, it properly resumes the study approach and the results.

INTRODUCTION: I appreciate the fact the authors go straight to the point of their research. In the first line of this section, it would be interesting if the authors should add some more references, such as:

Kulkova, M. A., Kashuba, M. T., Kulkov, A. M., Ryabkova, T. V., Vetrova, M. N., Zanoci, A., & Bubnova, O. V. (2022). Iron sources and technologies during the Early Iron Age in the Northern Pontic region. In Geoarchaeology and Archaeological Mineralogy: Proceedings of 7th Geoarchaeological Conference, Miass, Russia, 19–23 October 2020 (pp. 11-28). Springer International Publishing.

Shotten-Hallel, V., Ashkenazi, D., & Tal, O. (2022). Archaeometallurgical Analysis of Thirteenth-Century Bronze and Iron Construction Implements from the Walls of the Frankish Castle at Arsuf/Arsur. Metallography, Microstructure, and Analysis, 11(2), 255-280.

Marrocchino, E., Telloli, C., Finotti, S., Facchi, A., Eftekhari, N., & De Vito, C. (2022). Microstructure, Chemistry and Mineralogy Approach for the Diagnostics of Metallic Finds of the Tomba della Biga (Adria, Italy). Applied Sciences, 12(22), 11365.

Srivastava, N., Singh, A. K., Kanungo, A. K., Arora, A., Rajan, K., & Selvakumar, V. (2023). Comparative microstructural and elemental analysis of iron artefacts from Kaveri valley archaeological sites. Archaeometry, 65(6), 1246-1259.

 

MATERIALS AND METHODS: I appreciate the division in subparagraphs, where the authors well explain the archaeological setting, the sample preparation and the analytical methods they used.

RESULTS: are presented logically, with the data meticulously produced and thoroughly discussed. The high-quality images and diagrams significantly enhance the reader's comprehension of the text. The authors have effectively integrated various analytical techniques, which provide a comprehensive understanding of the microstructure..

DISCUSSION: The use of EBSD and Raman microspectroscopy for phase identification is particularly noteworthy, providing detailed insights into the composition and properties of the iron artefacts. The discussion section is well structured, linking the results to broader historical and metallurgical contexts, which enriches the relevance of the study. Overall, the clarity and thoroughness of the presentation make the article an excellent resource for researchers in the field. In my opinion, the authors extensively discuss the results obtained on the samples studied using different analytical methods. This section is well supported by appropriate evidence and provides good answers to the aims of the study.

CONCLUSION: The analysis provided in the study offers a comprehensive understanding of the manufacturing processes and material characteristics of Roman-period iron artefacts. By employing a multi-technique approach, including EBSD and microhardness measurements, the researchers effectively highlight the diverse metallurgical strategies employed by Roman blacksmiths.

Furthermore, the study's meticulous examination of non-metallic inclusions resulting from the bloomery process and their negligible impact on structural integrity provides valuable insights into the metallurgical quality control practices of the time.

In conclusion, the research significantly contributes to our knowledge of ancient metallurgy, showcasing the advanced skills and metallurgical knowledge possessed by Roman blacksmiths. However, further research could delve into the specific techniques used for carburization and decarburization, as well as explore the implications of these findings on broader archaeological interpretations of Roman iron artefacts.

 

I want to express my compliments on your study. I found the work elegantly and rationally presented, with interesting data providing the necessary background information and introducing the step-by-step approach of the study. It is well organised into appropriate sections, gets straight to the point and is easily understood by all types of readers

Author Response

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Author Response File: Author Response.pdf

Reviewer 2 Report

Comments and Suggestions for Authors

I enclose a draft with some comments to specific statements of the manuscript.

There are several points which are not well explained/constrained. I have simply highlighted words/sentences to be rewritten

Comments for author File: Comments.pdf

Comments on the Quality of English Language

The quality should be definitely improved

Author Response

Please see the attachment

Author Response File: Author Response.pdf

Round 2

Reviewer 2 Report

Comments and Suggestions for Authors I appreciate the efforts of the authors to improve the manuscript's quality by modifying the various weak points.   Comments on the Quality of English Language

Although I still recommend to check for the English style, the manuscript can now be accepted for publication